Thionyl Chloride → 2,4-Bis(dichloromethylidene)-2H,4H-1,3-benzodioxine-6-carbonitrile

HRID 224408노트

반응식

HRID 224408 반응식
[Cl:1][C:2]([Cl:19])=[C:3]1[O:8][C:7](=[C:9]([Cl:11])[Cl:10])[C:6]2[CH:12]=[C:13]([C:16]([NH2:18])=O)[CH:14]=[CH:15][C:5]=2[O:4]1.S(Cl)(Cl)=O>CN(C)C=O>[C:16]([C:13]1[CH:14]=[CH:15][C:5]2[O:4][C:3](=[C:2]([Cl:19])[Cl:1])[O:8][C:7](=[C:9]([Cl:11])[Cl:10])[C:6]=2[CH:12]=1)#[N:18]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 233329192,4-Bis(dichloromethylene)benzo[1,3]dioxin-6-carboxamide

생성물 1

HCID 233329162,4-Bis(dichloromethylidene)-2H,4H-1,3-benzodioxine-6-carbonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2,4-Bis(dichloromethylene)benzo[1,3]dioxin-6-carboxamide (3.0 g.) was added in portions to a stirred mixture of thionyl chloride (15 ml.) in dimethylformamide (60 ml.) at 50° C. A precipitate rapidly formed which, after cooling the reaction mixture to ambient temperature, was filtered off, dried, and crystallised from ethanol to give 6-cyano-2,4-bis(dichloromethylene)benzo[1,3]dioxin, m.p. 167°-168° C.

후처리

  1. customA precipitate rapidly formed which
  2. filtrationwas filtered off
  3. customdried
  4. customcrystallised from ethanol

출처 및 근거

ORD 기록
ord-063afedfb8db45b0b151fa0eee358d80
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04232032

반응 노트

불러오는 중…